反応 #92801

ord-2cfd64a566634aa5bc81b63d6e3f3d0a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過the resulting liquid was filtered
  2. 2
    その他to remove insoluble matters
  3. 3
    その他Thereafter, the obtained solution was subjected to separation operation
  4. 4
    洗浄the resulting methylene chloride solution was washed with a saturated aqueous sodium chloride solution
  5. 5
    乾燥dried over magnesium sulfate
  6. 6
    workup.DISTILLATIONAfter methylene chloride was distilled off
  7. 7
    洗浄the resulting solid matter was washed with methanol

実験手順

4-(benzyloxy)benzoic acid (20.0 g, 87.6 mmol), 4-(hexyloxy)phenol (17.0 g, 87.6 mmol), N,N′-dicyclohexylcarbodiimide (21.7 g, 105 mmol) and 4-dimethylaminopyridine (535 mg, 4.38 mmol) were dissolved in 300 mL of methylene chloride. The resulting solution was stirred for 3 hours at room temperature. Then, 300 mL of pure water was added thereto, and then the resulting liquid was filtered to remove insoluble matters. Thereafter, the obtained solution was subjected to separation operation, and the resulting methylene chloride solution was washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. After methylene chloride was distilled off, the resulting solid matter was washed with methanol. Thereby, a white solid compound, 4-(hexyloxy)phenyl 4-(benzyloxy)benzoate (24.9 g) was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09449732B2uspto-grants-2016_09